EP0571884B1 - Composite materials containing polyether ketone filaments - Google Patents

Composite materials containing polyether ketone filaments Download PDF

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Publication number
EP0571884B1
EP0571884B1 EP93108109A EP93108109A EP0571884B1 EP 0571884 B1 EP0571884 B1 EP 0571884B1 EP 93108109 A EP93108109 A EP 93108109A EP 93108109 A EP93108109 A EP 93108109A EP 0571884 B1 EP0571884 B1 EP 0571884B1
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EP
European Patent Office
Prior art keywords
yarn
folded
composite
cabled
threads
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Expired - Lifetime
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EP93108109A
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German (de)
French (fr)
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EP0571884A1 (en
Inventor
André Rötgers
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Invista Technologies SARL Switzerland
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Hoechst AG
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/902—High modulus filament or fiber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249922—Embodying intertwined or helical component[s]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249924—Noninterengaged fiber-containing paper-free web or sheet which is not of specified porosity
    • Y10T428/24994—Fiber embedded in or on the surface of a polymeric matrix
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
    • Y10T442/2861—Coated or impregnated synthetic organic fiber fabric
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/30—Woven fabric [i.e., woven strand or strip material]
    • Y10T442/3065—Including strand which is of specific structural definition

Definitions

  • the present invention relates to composite materials which contain threads or structures derived therefrom, such as threads or textile fabrics made of polyether ketones (hereinafter referred to as PEK).
  • PEK polyether ketones
  • Reinforcement yarns have already become known which have been textured by a blowing nozzle and have subsequently been embedded in a matrix material.
  • These are polyamide yarns, as known from US-A-3,314,897, or yarns from polyethylene terephthalate, as known from EP-A-319,940.
  • all of these materials can also be combined with the matrix using other methods, such as the use of adhesion promoters.
  • the object of the present invention is therefore to provide a composite material which contains PEK fibers as reinforcing materials and which is distinguished by excellent adhesion between the matrix material and the reinforcing material.
  • the invention relates to a composite material containing a polymeric organic compound as a matrix and threads or threads made of polyether ketone or textile fabrics constructed from these threads or threads as reinforcing material, characterized in that threads or threads made of polyether ketone which have a crimp are contained.
  • polyether ketones are understood to mean all polymers which have structural units -Ar-O- and -Ar-CO-, in which Ar stands for an aromatic radical. It can e.g. are a mono- or polynuclear aromatic hydrocarbon radical, in particular a phenylene radical. These structural units can be linked to one another in various ways, in particular in the p-position. According to common usage, the first unit is called “E” (ether) and the second unit is called “K” (ketone). depending on the sequence of the ether and ketone units, a distinction is made e.g. between PEK, PEEK, PEKK or PEEKK types. All of these types of polymers are included in the term polyether ketones for the purposes of this invention. The PEEK types are particularly preferably used.
  • All polymeric organic materials suitable for composite materials can be considered as matrix material.
  • This can be curable and / or thermoplastic, e.g. epoxy resins, curable polyester resins, melamine-formaldehyde resins, resols or novolaks or thermoplastic polyesters or thermoplastic aramids.
  • the matrix materials are particularly preferably elastomers, such as rubber or rubber.
  • the reinforcing material can be in the form of threads, twisted threads or textile fabrics made from them, such as knitted fabrics, knitted fabrics or, in particular, woven fabrics. It is essential that the PEK thread is crimped or that the structures derived therefrom, such as threads or fabric, contain such crimped threads. In the case of derived structures, it is sufficient if only a part of the threads building up these structures is crimped.
  • the PEK threads are made up of continuous filaments.
  • yarns made from crimped staple fibers can also be used.
  • the shape of the crimp can be any.
  • Blast-textured threads are preferably used, in particular those threads which have loops of filament capillaries.
  • the number of loops in these preferred threads is in particular 3 to 6 per cm of thread length.
  • the proportion of crimped threads is generally chosen so that the structure has practically no loss of strength compared to the structure composed only of smooth threads. In general, a proportion of less than 50% by weight of crimped threads, based on the weight of the structure, is sufficient.
  • the composite materials according to the invention based on elastomers can be used in particular as heat-resistant and chemical-resistant molded articles.
  • the adhesion of the thread was determined in N according to the T test by pulling it out of a rubber body of a defined size.
  • the adhesion values of the twine with textured content (25%) were 40% higher than the other two variants. When using adhesive mix, adhesive values are measured that are twice as high.
  • the elongation at break values are not affected. In both cases they are approximately 24%.

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  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Polymers & Plastics (AREA)
  • Manufacturing & Machinery (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Woven Fabrics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Reinforced Plastic Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Artificial Filaments (AREA)

Description

Die vorliegende Erfindung betrifft Verbundwerkstoffe, die Fäden oder davon abgeleitete Gebilde, wie Zwirne oder textile Flächengebilde aus Polyetherketonen (im folgenden PEK genannt) enthalten.The present invention relates to composite materials which contain threads or structures derived therefrom, such as threads or textile fabrics made of polyether ketones (hereinafter referred to as PEK).

Wie aus vielen Untersuchungen der letzten Jahre bekannt ist, besteht eine große Schwierigkeit bei der Einbettung von PEK-Garnen oder -Zwirnen darin, daß zwischen der PEK-Oberfläche und dem aufgetragenen Matrixmaterial eine gegenüber anderen Verstärkungsmaterialien, wie z.B. Polyamiden oder Polyestern nur sehr geringe Bindung zu erreichen ist. Dies ändert sich auch nicht oder kaum bei zusätzlicher Vorimprägnierung des PEK-Fadens mit den üblicherweise zur Verfügung stehenden Haftvermittlern auf Basis von Isocyanat-, Epoxid- oder Resorcinharz. Auch derart vorpräparierte Fäden ergeben eine, verglichen mit Polyamiden oder Polyestern, unzureichende Haftung. In der Praxis behilft man sich bislang mit Verstärkungskonstruktionen, die durch ihre offene Struktur einen Durchgriff des Matrixmaterials gestatten und dadurch eine mechanische Verankerung bewirken.As is known from many studies in recent years, a great difficulty with the embedding of PEK yarns or twists is that between the PEK surface and the applied matrix material there is a comparison with other reinforcing materials, e.g. Polyamides or polyesters only very low bond can be achieved. This does not change, or hardly changes, when the PEK thread is additionally pre-impregnated with the commonly available adhesion promoters based on isocyanate, epoxy or resorcinol resin. Threads prepared in this way also result in inadequate adhesion compared to polyamides or polyesters. In practice, reinforcement constructions have so far been used, which, due to their open structure, allow the matrix material to be penetrated and thereby cause mechanical anchoring.

Ursache der geringen Haftung ist der chemisch sehr neutrale Charakter von PEK, der eine chemische Bindung praktisch nicht zuläßt.The reason for the low adhesion is the chemically very neutral nature of PEK, which practically does not allow chemical bonding.

Es sind bereits Verstärkungsgarne bekannt geworden, die durch eine Blasdüse texturiert wurden und anschließend in ein Matrixmaterial eingebettet wurden. Dabei handelt es sich um Polyamidgarne, wie aus der US-A-3,314,897 bekannt, oder um Garne aus Polyethylenterephthalat, wie aus der EP-A-319,940 bekannt. Alle diese Materialien lassen sich, im Gegensatz zu PEK, auch mit anderen Methoden, wie Verwendung von Haftvermittlern, mit der Matrix verbinden.Reinforcement yarns have already become known which have been textured by a blowing nozzle and have subsequently been embedded in a matrix material. These are polyamide yarns, as known from US-A-3,314,897, or yarns from polyethylene terephthalate, as known from EP-A-319,940. In contrast to PEK, all of these materials can also be combined with the matrix using other methods, such as the use of adhesion promoters.

Aufgabe der vorliegenden Erfindung ist es daher, einen Verbundwerkstoff zur Verfügung zu stellen, der PEK-Fasern als Verstärkungsmaterialien enthält und der sich durch eine ausgezeichnete Haftung zwischen Matrixmaterial und Verstärkungsmaterial auszeichnet.The object of the present invention is therefore to provide a composite material which contains PEK fibers as reinforcing materials and which is distinguished by excellent adhesion between the matrix material and the reinforcing material.

Die Erfindung betrifft einen Verbundwerkstoff enthaltend als Matrix eine polymere organische Verbindung und als Verstärkungsmaterial Fäden oder Zwirne aus Polyetherketon oder aus diesen Fäden oder Zwirnen aufgebaute textile Flächengebilde, dadurch gekennzeichnet, daß Fäden oder Zwirne aus Polyetherketon die eine Kräuselung aufweisen enthalten sind.The invention relates to a composite material containing a polymeric organic compound as a matrix and threads or threads made of polyether ketone or textile fabrics constructed from these threads or threads as reinforcing material, characterized in that threads or threads made of polyether ketone which have a crimp are contained.

Unter Polyetherketonen (PEK) werden im Rahmen dieser Erfindung alle Polymere verstanden, die Struktureinheiten -Ar-O- und -Ar-CO- aufweisen, worin Ar für einen aromatischen Rest steht. Dabei kann es sich z.B. um einen ein- oder mehrkernigen aromatischen Kohlenwasserstoffrest handeln, insbesondere um einen Phenylenrest. Diese Struktureinheiten können auf verschiedene Art miteinander verknüpft sein, insbesondere in p-Stellung. Gemäß dem allgemeinen Sprachgebrauch bezeichnet man die erste Einheit als "E" (Ether) und die zweite Einheit als "K" (Keton). je nach Abfolge der Ether- und Ketoneinheiten unterscheidet man z.B. zwischen PEK-, PEEK-, PEKK- oder PEEKK-Typen. Alle diese Polymertypen sind vom Begriff Polyetherketone im Sinne dieser Erfindung umfaßt. Besonders bevorzugt verwendet man die PEEK-Typen.In the context of this invention, polyether ketones (PEK) are understood to mean all polymers which have structural units -Ar-O- and -Ar-CO-, in which Ar stands for an aromatic radical. It can e.g. are a mono- or polynuclear aromatic hydrocarbon radical, in particular a phenylene radical. These structural units can be linked to one another in various ways, in particular in the p-position. According to common usage, the first unit is called "E" (ether) and the second unit is called "K" (ketone). depending on the sequence of the ether and ketone units, a distinction is made e.g. between PEK, PEEK, PEKK or PEEKK types. All of these types of polymers are included in the term polyether ketones for the purposes of this invention. The PEEK types are particularly preferably used.

Als Matrixmaterial kommen alle für Verbundwerkstoffe geeigneten polymeren organischen Materialien in Betracht. Dabei kann es sich um härtbare und/oder um thermoplastische Kunststoffe handeln, wie z.B. um Epoxidharze, härtbare Polyesterharze, Melamin-Formaldehydherze, Resole oder Novolake oder um thermoplastische Polyester oder um thermoplastische Aramide.All polymeric organic materials suitable for composite materials can be considered as matrix material. This can be curable and / or thermoplastic, e.g. epoxy resins, curable polyester resins, melamine-formaldehyde resins, resols or novolaks or thermoplastic polyesters or thermoplastic aramids.

Besonders bevorzugt handelt es sich bei den Matrixmaterialien um Elastomere, wie Kautschuk oder Gummi.The matrix materials are particularly preferably elastomers, such as rubber or rubber.

Das Verstärkungsmaterial kann in Form von Fäden, Zwirnen oder daraus aufgebauten textilen Flächengebilden, wie Gestricken, Gewirken oder insbesondere Geweben, vorliegen.
Wesentlich ist, daß der PEK-Faden gekräuselt ist oder daß die daraus abgeleiteten Strukturen, wie Zwirne oder Gewebe solche gekräuselten Fäden enthalten. Bei abgeleiteten Strukturen reicht es aus, wenn lediglich ein Teil der diese Strukturen aufbauenden Fäden gekräuselt ist.The reinforcing material can be in the form of threads, twisted threads or textile fabrics made from them, such as knitted fabrics, knitted fabrics or, in particular, woven fabrics.
It is essential that the PEK thread is crimped or that the structures derived therefrom, such as threads or fabric, contain such crimped threads. In the case of derived structures, it is sufficient if only a part of the threads building up these structures is crimped.

Im allgemeinen sind die PEK-Fäden aus Endlosfilamenten aufgebaut. Es lassen sich aber auch Garne aus gekräuselten Stapelfasern verwenden.In general, the PEK threads are made up of continuous filaments. However, yarns made from crimped staple fibers can also be used.

Die Form der Kräuselung kann beliebig sein. So kann es sich z.B. um zahnradgekräuselte oder um stauchkammergekräuselte Fäden handeln. Vorzugsweise verwendet man blastexturierte Fäden, insbesondere solche Fäden, die Schlaufen aus Filamentkapillaren aufweisen.The shape of the crimp can be any. For example, be gear crimped or stuffer box crimped threads. Blast-textured threads are preferably used, in particular those threads which have loops of filament capillaries.

Die Schlaufenzahl beträgt bei diesen bevorzugten Fäden insbesondere 3 bis 6 pro cm Fadenlänge.The number of loops in these preferred threads is in particular 3 to 6 per cm of thread length.

Besonders bevorzugt verwendet man Zwirne oder Gewebe aus glatten und gekräuselten PEK-Fäden. Dabei wählt man den Anteil der gekräuselten Fäden im allgemeinen so, daß die Struktur praktisch keinen Festigkeitsverlust gegenüber der nur aus glatten Fäden aufgebauten Struktur aufweist. Im allgemeinen genügt ein Anteil von weniger als 50 Gew.-% an gekräuselten Fäden, bezogen auf das Gewicht der Struktur.It is particularly preferred to use threads or fabrics made of smooth and crimped PEK threads. The proportion of crimped threads is generally chosen so that the structure has practically no loss of strength compared to the structure composed only of smooth threads. In general, a proportion of less than 50% by weight of crimped threads, based on the weight of the structure, is sufficient.

Die erfindungsgemäßen Verbundwerkstoffe auf der Basis von Elastomeren lassen sich insbesondere als hitze- und chemikalienbeständige Formkörper einsetzen.The composite materials according to the invention based on elastomers can be used in particular as heat-resistant and chemical-resistant molded articles.

Das nachfolgende Beispiel erläutert die Erfindung.The following example explains the invention.

Beispiel 1example 1

Bei einem Versuch wurde ein Fadenanteil der zu einem PEK-Zwirn der Konstruktion (dtex 410 x 4) x 2 benötigten Filamente durch einen blastexturierten dtex 410-Faden ersetzt. Die Konstruktion sah danach folgendermaßen aus:

Figure imgb0001
In one test, a thread portion of the filaments required for a PEK thread of construction (dtex 410 x 4) x 2 was replaced by a blast textured dtex 410 thread. The construction then looked like this:
Figure imgb0001

Dieser Zwirn wurde in Gummimischung ohne zusätzlichen Haftvermittler einvulkanisiert. Verglichen wurde das Haftergebnis mit Zwirnen

  • a) aus 100 % glattem Material und
  • b) aus glattem Material, welches mit RFL (Resorcin-Formaldehyd Latex) vorimprägniert wurde.
This thread was vulcanized into a rubber mixture without an additional adhesion promoter. The detention result was compared with twine
  • a) 100% smooth material and
  • b) made of smooth material, which was pre-impregnated with RFL (resorcinol-formaldehyde latex).

Die Haftung des Zwirnes wurde in N gemäß T-Test durch Herauszsiehen aus einem Gummikörper definierter Größe ermittelt.The adhesion of the thread was determined in N according to the T test by pulling it out of a rubber body of a defined size.

Die Haftwerte des Zwirns mit texturiertem Anteil (25 %) fielen gegenüber den beiden anderen Varianten um 40 % höher aus. Bei Einsatz von Haftmischung werden sogar über doppelt so hohe Haftwerte gemessen.The adhesion values of the twine with textured content (25%) were 40% higher than the other two variants. When using adhesive mix, adhesive values are measured that are twice as high.

Der durch den Einsatz blastexturierten Materials bedingte Festigkeitsabfall (ausgedrückt in Höchstzugkraft HZK) des unbeschichteten Zwirns hält sich in Grenzen, wenn nur ein Teil des Zwirns aus einem texturierten Faden besteht: PEK-Zwirn 100 % glatt HZK = 188,01 (N) PEK-Zwirn 75 % glatt 25 % text HZK = 165,06 (N). The drop in strength of the uncoated thread caused by the use of blast-textured material (expressed in maximum tensile strength HZK) is limited if only part of the thread consists of a textured thread: PEK thread 100% smooth HZK = 188.01 (N) PEK thread 75% smooth 25% text HZK = 165.06 (N).

Die Bruchdehnungswerte werden nicht beeinflußt. Sie betragen in beiden Fällen ca. 24 %.The elongation at break values are not affected. In both cases they are approximately 24%.

Claims (8)

  1. A composite matrix comprising a polymeric organic compound and a reinforcing material comprising a polyether ketone single, folded or cabled yarn or a fabric formed from such single, folded or cabled yarn, characterized in that crimped polyether ketone single, folded or cabled yarn is comprised.
  2. The composite of claim 1, characterized in that the polymeric organic matrix material is rubber.
  3. The composite of claim 1, characterized in that the polymeric organic matrix material is a curable and/or thermoplastic synthetic resin.
  4. The composite of claim 1, characterized in that the reinforcing material comprises stuffer box textured single yarn or is folded or cabled yarn comprising such single yarn or woven fabric comprising such single, folded or cabled yarn.
  5. The composite of claim 1, characterized in that the reinforcing material comprises air jet textured single yarn with loops or is folded or cabled yarn comprising such single yarn or woven fabric comprising such single, folded or cabled yarn.
  6. The composite of claim 5, characterized in that the number of loops is from 3 to 6 per cm of the yarn.
  7. The composite of claim 1, characterized in that the reinforcing material is folded or cabled yarn comprising textured and flat single yarns and the proportion of textured single yarn based on the weight of the reinforcing material is less than 50% by weight.
  8. The use of crimped polyether ketone yarn for reinforcing organic polymer materials, in particular for reinforcing rubber.
EP93108109A 1992-05-27 1993-05-18 Composite materials containing polyether ketone filaments Expired - Lifetime EP0571884B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4217475 1992-05-27
DE4217475 1992-05-27

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EP0571884B1 true EP0571884B1 (en) 1997-04-02

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US (1) US5342677A (en)
EP (1) EP0571884B1 (en)
JP (1) JPH0649237A (en)
CA (1) CA2097031A1 (en)
DE (1) DE59306007D1 (en)
FI (1) FI932371A (en)
NO (1) NO931916L (en)

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DE19624235C2 (en) * 1996-06-18 1999-04-08 Contitech Luftfedersyst Gmbh Composite material

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* Cited by examiner, † Cited by third party
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DE3881230T2 (en) * 1987-02-20 1993-10-07 Albany Int Corp Artificial down.
JPH0817880B2 (en) * 1990-11-28 1996-02-28 帝人株式会社 Press cushion material
US5227236A (en) * 1991-07-29 1993-07-13 Basf Aktiengesellschaft Process for preparing thermoplastic matrix fiber-reinforced prepregs and composite structure products formed thereby
US5225265A (en) * 1991-12-06 1993-07-06 Basf Aktiengesellschaft Environmentally durable lightning strike protection materials for composite structures

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NO931916L (en) 1993-11-29
US5342677A (en) 1994-08-30
JPH0649237A (en) 1994-02-22
EP0571884A1 (en) 1993-12-01
FI932371A (en) 1993-11-28
CA2097031A1 (en) 1993-11-28
FI932371A0 (en) 1993-05-25
DE59306007D1 (en) 1997-05-07
NO931916D0 (en) 1993-05-26

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